A series of polyethers were prepared by polycondensation reaction between bisphenolate anions and 1,6-dibromohexane in the two phase, heterogeneous system of water and nitrobenzene. Dibenzo-18-crown-6 was employed as a phase transfer catalyst. Of the alkali metal salts examined (Li⁺, Na⁺, K⁺, and Cs⁺) phase transfer activity was found to be at a maximum when the counter cation of bisphenolate was K⁺. Activity of dibenzo-18-crown-6 appeared to be less effective for this particular reaction than that of tetrabutylammonium bromide. Reactivity of bisphenolate anions decreased in the order : 2,2-bis(4-hydroxyphenyl) propane > bis(4-hydroxyphenyl) sulfide > bis(4-hydroxyphenyl) ketone > bis(4-hydroxyphenyl) sulfone. Employment of excess amount. of potassium hydroxide facilitated the transfer of bisphenolate anions from the aqueous to the nitrobenzene phase,thus increasing the polycondensation rate.